Diacetyl has been identified from its retention time by gas chromatography in condensates of the vapor collected from the model dough which was baked in a flask heated in an oil bath at 130°C for 60min. The dough was prepared by mixing 8g of flour, 2g of cane sugar, 2g of butter, 20 mg of NaHCO3 and 2ml of water. Diacetyl was found as one of the characteristic, pleasant aroma components of biscuit by sensory test. In the analysis of vapor sample evolved from baked biscuit by gas chromatography, diacetyl formation increased with prolongation of baking time, with raise of the pH of dough, and with increasing in the amount of cane sugar used in the dough. Although diacetyl was considered to be derived from the sugar, diacetyl formation was not remarkable in the case of using cane sugar or flour only. But diacetyl was distinctly produced in the presence of the flour when mixed with cane sugar. It was considered that diacetyl might be developed during the baking process, in which the browning reaction of wheat flour and cane sugar occurred in dough.